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1-Bromopropane → HCID 178460859、化合物

HRID 1757168
ノート
印刷プレビュー

反応式

HRID 1757168 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][NH:9][C:10]([NH2:12])=[S:11].[CH2:13](Br)[CH2:14][CH3:15]>C(#N)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][NH:9][C:10](=[NH:12])[S:11][CH2:13][CH2:14][CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 78401-BromopropaneHCID 22400378HCID 22400378、化合物

生成物 1

HCID 178460859HCID 178460859、化合物収率 78%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 1-(2-chlorophenyl)methyl thiourea (3 g, 14.9 mmol) and propylbromide (13.5 g, 110 mmol) in acetonitrile (20 mL) was refluxed for 5 hours. The solvent was evaporated, the residue was dissolved in 200 mL of 50% water/ether and acidified with 48% hydrobromic acid solution. The two phases were separated, the aqueous layer was washed with ether and then the aqueous layer was basified with 10% sodium carbonate solution. The liberated product was extracted with diethyl ether, washed with water and brine, dried and concentrated to give 1-(2-chlorophenyl)methyl-2-propyl-2-thiopseudourea (2.82 g, 78%); mp 112°-114° C.

後処理

  1. temperaturewas refluxed for 5 hours
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in 200 mL of 50% water/ether
  4. customThe two phases were separated
  5. washthe aqueous layer was washed with ether
  6. extractionThe liberated product was extracted with diethyl ether
  7. washwashed with water and brine
  8. customdried
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-354a05fc5b144785ab7ce3fd07a38d06
出典データセット
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05444080

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート